CN112080247B - Water-based silicone adhesive capable of bonding RTV silicone adhesive - Google Patents
Water-based silicone adhesive capable of bonding RTV silicone adhesive Download PDFInfo
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- CN112080247B CN112080247B CN202010909533.7A CN202010909533A CN112080247B CN 112080247 B CN112080247 B CN 112080247B CN 202010909533 A CN202010909533 A CN 202010909533A CN 112080247 B CN112080247 B CN 112080247B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
Abstract
The invention discloses a bondable RTV silicone adhesive with good thixotropy, which mainly comprises 50-120 parts of 30-80% hydroxyl silicone oil emulsion, 0.1-5 parts of a cross-linking agent, 0.2-5 parts of a silane coupling agent, 0.01-1 part of a catalyst, 1-10 parts of precipitated white carbon black, 1-10 parts of fumed white carbon black, 1-50 parts of ground calcium carbonate and 1-100 parts of silicon micropowder, wherein the cross-linking agent, the silane coupling agent and the catalyst are respectively selected from specific components. The water-based silicone adhesive can be directly coated on the mildewed and yellowed RTV silicone adhesive; the coating has thixotropy, can be coated on a vertical surface or a top lower surface, and cannot generate a sagging phenomenon; the surface drying time is slow, and if the glue is applied wrongly, the glue can be conveniently removed by a rag with water; the adhesive property is strong, the system is stable, the performance is excellent, and the shelf life is long; simple manufacture, no toxicity, no harm, no emission, green and environmental protection. The invention also discloses the application of the water-based silicone adhesive as a renovation adhesive of the mildewed or yellowed RTV silicone adhesive and a preparation method thereof.
Description
Technical Field
The invention relates to the field of silicone adhesive, in particular to water-based silicone adhesive, and especially relates to water-based silicone adhesive capable of bonding RTV silicone adhesive.
Background
RTV Silicone adhesive is a room temperature vulcanized silicone rubber, RTV is an abbreviation for room temperature vulcanized silicone rubber, and the base stock is 107 silicone rubber, known under the chemical name alpha, omega-dihydroxy polydimethylsiloxane. The RTV silicone adhesive is paste in appearance, is prepared by compounding silicone rubber, a cross-linking agent, a filler and the like, has long storage period and stable performance, is generally used for bonding and sealing substrates such as glass, aluminum materials, ceramic tiles and the like, and is suitable for bonding and sealing among various metals and between metal and non-metal materials.
RTV silicone adhesive bonds with the substrate and solidifies through the mode of moisture solidification, and its bonding effect is very good, but the glue itself can be very thick, will generally add plasticizer such as white oil/silicone oil to improve extrudability, meanwhile, long time, the glue after solidifying easily bleeds oil and pollutes the substrate, easy yellowing (such as the glueing department such as toilet in the home, bathroom easily becomes yellow and even blackens), influences the appearance, can even go moldy and need to shovel off and reapply glueing. Because the RTV silicone adhesive has better bonding property and is very inconvenient to remove and glue, the development of renovating adhesive which can be directly coated on the yellowing and mildewed RTV silicone adhesive, is firmly bonded with the RTV silicone adhesive and can beautify the renovating RTV silicone adhesive is urgently needed.
The RTV silicone adhesive begins to react and solidify when meeting water vapor in the air, thereby playing a role in bonding or sealing, being oil-based or solvent-free and being incapable of bonding wet base materials; the environment is not protected, and small molecular organic compounds (VOCs) can be released in the vulcanization process to pollute the environment and cause certain damage to the bodies of constructors; the environment is polluted due to improper construction in the construction process and is difficult to remove; and the glue after curing is easy to seep oil and pollute the base material and turn yellow easily after a long time, which affects the appearance. In order to overcome the defects of the RTV silicone adhesive, the development of the water-based silicone adhesive with more excellent performance and larger market prospect is needed.
At present, the records of the water-based silicone adhesive in China are less, and the 'water-based silicone adhesive' of the network search shows that the 'water-based silicone adhesive' is basically water-based acrylic adhesive and does not stick RTV silicone adhesive at all. Only a few documents describing the water-based silicone adhesive can be found, such as "development of low modulus high elongation room temperature vulcanized water-based silicone sealant" (Pengzoli et al, proceedings of the Huizhou academy of academic, 2005,025(003):1-6) "," preparation of water-dispersible RTV-1 silicone sealant for road joints "(Qiuhao et al, silicone material, 2007,21 (6): 329-331)", "research on adhesion of room temperature vulcanized water-based silicone rubber" (Pengzoli et al, chemical adhesion, 2005,27 (4): 200-205) ", and domestic patent ZL200710049060.2, but the water-based silicone adhesive is mainly used for sealing expansion joints of buildings and expansion joints of concrete pavements, and does not mention the problems of adhesion and thixotropy of the water-based silicone adhesive to RTV silicone adhesive, and the water-based silicone adhesive prepared by the prior art is difficult to be coated on the water-based silicone adhesive due to the low surface energy of the RTV silicone adhesive, the emulsion is unstable and easy to agglomerate due to no selection of proper cross-linking agent, coupling agent and catalyst, and has poor adhesion to RTV silicone adhesive and short shelf life; meanwhile, proper filler is not selected, or only white carbon black is adopted, so that the thixotropy is poor, and a sagging phenomenon can be generated when the white carbon black is coated on a vertical surface or a top lower surface.
Disclosure of Invention
In order to solve the above problems, the present invention provides an aqueous silicone adhesive which can bond RTV silicone adhesives, has good thixotropy, and can be used as a retread adhesive for mildewed or yellowed RTV silicone adhesives.
The water-based silicone adhesive provided by the invention comprises, by mass, 50-120 parts of 30% -80% hydroxyl silicone oil emulsion, 0.1-5 parts of a cross-linking agent, 0.2-5 parts of a silane coupling agent, 0.01-1 part of a catalyst and a filler.
Wherein the silane coupling agent is one or more selected from 3-glycidoxypropyltrimethoxysilane, (3-glycidoxypropyl) methyldimethoxysilane, 3-aminopropyltriethoxysilane, 2-dimethoxy-1, 6-diaza-2-silacyclooctane, 3-aminopropylmethyldiethoxysilane, N- (2-aminoethyl) -aminopropylmethyldimethoxysilane, N- (2-aminoethyl) -aminopropyltrimethoxysilane and N- (2-aminoethyl) -aminopropyltriethoxysilane.
The silane coupling agent of the invention mainly plays a role in binding and stabilizing a system. When the cross-linking agent and the silane coupling agent meet and react, the silane coupling agent plays a role in bonding, so that the bonding property is stronger. The system is not stable enough when the silane coupling agent is not added, the system can be damaged sometimes, the glue is directly cured in the preparation process, and even if the glue can be prepared, the base materials such as aluminum sheets and the like can not be adhered after curing.
The silane coupling agent selected by the invention is water-soluble silane coupling agent, so that the silane coupling agent can not react with the crosslinking agent dispersed in the oil phase when the moisture is not completely volatilized, and can react with the crosslinking agent after the moisture is completely volatilized.
Generally, the hydroxyl silicone oil emulsion is anionic or nonionic, and the existing crosslinking agent and coupling agent are neutral and are not easy to disperse charges, so that the emulsion cannot be stabilized. The silane coupling agent of the invention is slightly alkaline and can be dispersed in water to just play a role in stabilizing emulsion.
Through a large number of experiments, the silane coupling agent with more than 8 components is selected from a variety of water-based silane coupling agents and is used for preparing the water-based silicone adhesive, and the selected silane coupling agent and the cross-linking agent can be perfectly matched with the hydroxyl silicone oil emulsion, so that the performance of the prepared water-based silicone adhesive is greatly improved, and the RTV silicone adhesive is more effectively bonded.
Further, the silane coupling agent is 3-glycidoxypropyltrimethoxysilane.
Further, the cross-linking agent is one or more selected from styrene ethyl methyl dimethoxy silane, styrene ethyl triethoxy silane, vinyl trimethoxy silane, vinyl triethoxy silane, vinyl methyl diethoxy silane, methyl trimethoxy silane, methyl ethyl dimethoxy silane and methyl triethoxy silane.
The cross-linking agent selected by the invention is oily and is dispersed in the oil phase. The cross-linking agent can be cross-linked with the hydroxyl silicone oil to generate a network structure, so that the strength of the glue after curing is provided. Through a large number of experiments, the cross-linking agent with the above 8 components is selected from a variety of oily cross-linking agents and is used for preparing the water-based silicone adhesive.
In the existing preparation process of the water-based silicone adhesive, an oily cross-linking agent and a coupling agent are generally adopted, so that the cross-linking agent and the coupling agent are only dispersed in an emulsion, the emulsion is easy to be unstable and to be demulsified, and even after a filler is added, a system is directly agglomerated. The silane coupling agent selected by the invention is water-soluble silane coupling agent, so that the silane coupling agent can not react with the crosslinking agent dispersed in the oil phase when the moisture is not completely volatilized, and can react with the crosslinking agent after the moisture is completely volatilized.
If the cross-linking agent and the coupling agent are both in the oil phase, the shelf life of the glue is short, and the cross-linking agent and the water-based silane coupling agent are respectively dispersed in the oil phase and the water phase, so that the cross-linking agent and the water-based silane coupling agent are prevented from meeting each other in advance, and the shelf life is greatly prolonged.
The surface energy of the cured RTV silicone adhesive is low and the waterborne silicone adhesives prepared by the prior art are difficult to coat. The water-based silane coupling agent adopted by the invention has better adhesion and can be matched with a small amount of hydroxyl and certain organic groups on the surface of the cured RTV silicone adhesive. Therefore, the crosslinking agent and the silane coupling agent selected by the invention are matched with the hydroxyl silicone oil emulsion to prepare the waterborne silicone adhesive which can effectively bond and solidify RTV silicone adhesive and can also bond with various substrates such as aluminum sheets, ceramic tiles and the like. Experiments show that: when the aqueous silicone adhesive prepared by the invention is coated on the cured RTV silicone adhesive, after the curing is complete, cohesive failure occurs, and the adhesion is good.
Further, the cross-linking agent is styrene ethyl triethoxysilane.
Further, the catalyst is one or more selected from dibutyl tin dilaurate, tetrabutyl titanate, diisopropyl di (ethyl acetoacetate) titanate and titanium complex.
The catalyst can accelerate the reaction and curing of the system. The catalyst selected by the invention is oily, is dispersed in an oil phase, cannot react with the silane coupling agent when the moisture is not completely volatilized, and can play a role in accelerating the curing of a system after the moisture is completely volatilized.
Through a large number of experiments, the catalyst with the above 4 components is selected from a variety of oily catalysts and is used for preparing the water-based silicone adhesive, the selected catalyst can be perfectly matched with a silane coupling agent, a cross-linking agent and a hydroxyl silicone oil emulsion, and the performance of the prepared water-based silicone adhesive is greatly improved.
Therefore, in the system provided by the invention, the cross-linking agent is oily, the silane coupling agent is aqueous, and the catalyst is oily. Therefore, the cross-linking agent and the catalyst are dispersed in the oil phase, and the silane coupling agent is dispersed in the water phase and has better protection effect on the emulsion. Their properties ensure that they do not meet in emulsion systems, but only when the moisture has evaporated, the system achieves a cured bond. Therefore, the water-based silicone adhesive obtained by the invention has slow surface drying time, and can be conveniently removed by a water-carrying rag if the glue is applied wrongly. Meanwhile, as the specific water-based silane coupling agent, cross-linking agent and catalyst are adopted, the system is more stable, the cohesiveness is good, the RTV silicone adhesive can be firmly bonded, and the RTV silicone adhesive can be used as a renovation adhesive of the RTV silicone adhesive.
Further, the catalyst is diisopropyl di (ethyl acetoacetate) titanate.
Further, the filler is 1-10 parts of precipitated white carbon black, 1-10 parts of gas-phase white carbon black, 1-50 parts of ground calcium carbonate and 1-100 parts of silica powder.
The filler adopted by the invention comprises precipitated white carbon black, gas-phase white carbon black, precipitated white carbon black, ground limestone and silicon micropowder. The precipitated white carbon black and the fumed white carbon black can play a role of a thickening agent, and the important point is that the prepared water-based silicone adhesive has good thixotropy and is not easy to crack after being cured by adjusting the proportion (experiments show that the fumed white carbon black which is used independently has excellent thixotropy but the adhesive is easy to crack after being cured, and the precipitated white carbon black which is added independently has no thixotropy); the ground calcium carbonate here acts as an extender; the fine silica powder plays a role in increasing the hardness. The four fillers are subjected to multiple tests to obtain the optimal mass ratio, so that the prepared water-based silicone adhesive has more appropriate thixotropy and hardness and more excellent performance.
Further, the mass ratio of the precipitated white carbon black to the fumed white carbon black is 5 parts: and 2 parts.
Although the gas phase white carbon black used alone is excellent in thixotropy, the glue is easy to crack after being cured; the precipitated white carbon black is added independently, so that the thixotropy is avoided. Meanwhile, the precipitated white carbon black and the fumed white carbon black are adopted and adjusted to be in a proper mass ratio, so that the consistency of the waterborne silicone adhesive can be ensured, the waterborne silicone adhesive has better thixotropy, and the cured waterborne silicone adhesive is not easy to crack, therefore, the prepared waterborne silicone adhesive can be coated on the vertical surface or the top lower surface of the RTV silicone adhesive, and the sagging phenomenon cannot be caused. Experiments prove that the mass ratio of the precipitated white carbon black to the gas-phase white carbon black is 5 parts: the best effect is achieved when 2 parts of the active ingredients are used.
Further, the water-based silicone adhesive comprises 100 parts of 30-80% hydroxyl silicone oil emulsion, 1 part of cross-linking agent, 2 parts of silane coupling agent, 0.5 part of catalyst, 5 parts of precipitated white carbon black, 2 parts of gas-phase white carbon black, 10 parts of ground calcium carbonate and 20 parts of silicon micropowder.
Further, the water-based silicone adhesive may further include a toner and/or a mildewproof agent.
Further, the aqueous silicone adhesive may further include a pigment. Different pigments can be added according to the desired color.
Further, the pigment is one or more of titanium dioxide, iron oxide red and iron oxide yellow.
Furthermore, the waterborne silicone adhesive can be added with a mildew inhibitor, and different mildew inhibitors can be added according to mildew prevention requirements.
In another aspect, the invention also provides the use of a mixture in the preparation of a retreaded adhesive for bonding RTV silicone adhesive, the mixture comprising 50-120 parts of 30-80% hydroxyl silicone oil emulsion, 0.1-5 parts of cross-linking agent, 0.2-5 parts of silane coupling agent, 0.01-1 part of catalyst and filler; wherein the silane coupling agent is one or more selected from 3-glycidoxypropyltrimethoxysilane, (3-glycidoxypropyl) methyldimethoxysilane, 3-aminopropyltriethoxysilane, 2-dimethoxy-1, 6-diaza-2-silacyclooctane, 3-aminopropylmethyldiethoxysilane, N- (2-aminoethyl) -aminopropylmethyldimethoxysilane, N- (2-aminoethyl) -aminopropyltrimethoxysilane, and N- (2-aminoethyl) -aminopropyltriethoxysilane; the preparation method of the mixture comprises the following steps of firstly, adding a cross-linking agent into the hydroxyl silicone oil emulsion, and stirring; then adding a coupling agent and stirring; adding a catalyst and stirring; adding precipitated white carbon black and gas-phase white carbon black, stirring and defoaming; and finally adding heavy calcium carbonate and silica micropowder, stirring and defoaming.
The water-based silicone adhesive prepared by the invention has excellent performances of being capable of bonding RTV silicone adhesive, having good thixotropy, being capable of being used as renovation adhesive of mildewed or yellowed RTV silicone adhesive and the like, and the main reason is that the cross-linking agent, the silane coupling agent, the catalyst, the filler and the hydroxyl silicone oil emulsion are perfectly matched in the preparation method. Through a large number of experiments, the invention selects the most appropriate reagents from a plurality of crosslinking agents, silane coupling agents, catalysts and fillers, and is suitable for the invention.
In conclusion, the invention provides the water-based silicone adhesive which can be used for bonding the RTV silicone adhesive, has good thixotropy, can be used as a renovation adhesive of mildewed or yellowed RTV silicone adhesive, and mainly has the following beneficial effects:
1. the coating can be directly coated on the mildewed and yellowed RTV silicone adhesive, and because of different systems, the mildewed and yellowed RTV silicone adhesive does not influence new adhesives, and is very convenient. In some cases where the silicone adhesive breaks, the adhesive made by the method can also be repaired.
2. Has thixotropy, can be coated on vertical surfaces or top and bottom surfaces, and does not generate sagging phenomenon.
3. The tack-free time is slow and, in the event of an incorrect application, can be easily removed with a water-carrying wipe.
4. Strong cohesiveness, stable system, excellent performance and long shelf life.
5. The preparation method is simple, nontoxic, harmless, emission-free and environment-friendly.
6. The color can be adjusted according to the requirement, and the mildew preventive is added according to the mildew prevention requirement to achieve the corresponding mildew prevention effect.
Detailed Description
The present invention is described in further detail below with reference to examples, which are intended to facilitate the understanding of the present invention without limiting it in any way. The reagents used in this example were all known products and were obtained by purchasing commercially available products.
EXAMPLE 11 parts of crosslinker styrene Ethyl triethoxysilane
The preparation method of the water-based silicone adhesive comprises the steps of firstly adding 1 part of styrene ethyl triethoxysilane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
EXAMPLE 24 parts of crosslinker styrene Ethyl triethoxysilane
The preparation method of the water-based silicone adhesive comprises the following steps of firstly adding 4 parts of styrene ethyl triethoxysilane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
EXAMPLE 31 parts of Cross-linking agent styrene Ethyl triethoxysilane +2 parts of silane coupling agent 3-glycidoxypropyltrimethoxysilane
The preparation method of the water-based silicone adhesive comprises the steps of firstly adding 1 part of styrene ethyl triethoxysilane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then adding 2 parts of 3-glycidoxypropyltrimethoxysilane, and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
EXAMPLE 41 parts of Cross-linking agent styrene Ethyl triethoxysilane +2 parts of oily coupling agent Gamma-methacryloxypropyl trimethoxysilane
The preparation method of the water-based silicone adhesive comprises the steps of firstly adding 1 part of styrene ethyl triethoxysilane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then adding 2 parts of gamma-methacryloxypropyl trimethoxy silane, and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
EXAMPLE 51 parts of Cross-linking agent styrene Ethyl triethoxysilane +2 parts of silane coupling agent N- (2-aminoethyl) -aminopropyl methyldimethoxysilane
The preparation method of the water-based silicone adhesive comprises the steps of firstly adding 1 part of styrene ethyl triethoxysilane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then adding 2 parts of N- (2-aminoethyl) -aminopropylmethyldimethoxysilane and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
EXAMPLE 61 parts of Cross-linking agent styrene Ethyl triethoxysilane +2 parts of silane coupling agent (3-glycidoxypropyl) methyldimethoxysilane
The preparation method of the water-based silicone adhesive comprises the steps of firstly adding 1 part of styrene ethyl triethoxysilane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then adding 2 parts of (3-glycidoxypropyl) methyldimethoxysilane, and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
EXAMPLE 71 parts crosslinker styrene Ethyl triethoxysilane +2 parts silane coupling agent 3-aminopropyl triethoxysilane
The preparation method of the water-based silicone adhesive comprises the steps of firstly adding 1 part of styrene ethyl triethoxysilane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then adding 2 parts of 3-aminopropyltriethoxysilane, and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
EXAMPLE 81 parts of the crosslinking agent styrene ethyltriethoxysilane +2 parts of the silane coupling agent 2, 2-dimethoxy-1, 6-diaza-2-silacyclooctane
The preparation method of the water-based silicone adhesive comprises the steps of firstly adding 1 part of styrene ethyl triethoxysilane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then adding 2 parts of 2, 2-dimethoxy-1, 6-diaza-2-silacyclooctane, and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
EXAMPLE 91 parts crosslinker styrene Ethyl triethoxysilane +2 parts silane coupling agent 3-aminopropyl methyl diethoxysilane
The preparation method of the water-based silicone adhesive comprises the steps of firstly adding 1 part of styrene ethyl triethoxysilane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then adding 2 parts of 3-aminopropyl methyl diethoxy silane and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
EXAMPLE 101 parts of a crosslinking agent styrene ethyltriethoxysilane +2 parts of a silane coupling agent N- (2-aminoethyl) -aminopropyltrimethoxysilane
The preparation method of the water-based silicone adhesive comprises the steps of firstly adding 1 part of styrene ethyl triethoxysilane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then adding 2 parts of N- (2-aminoethyl) -aminopropyltrimethoxysilane and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
EXAMPLE 111 parts of Cross-linking agent styrene Ethyl triethoxysilane +2 parts of silane coupling agent N- (2-aminoethyl) -aminopropyl triethoxysilane
The preparation method of the water-based silicone adhesive comprises the steps of firstly adding 1 part of styrene ethyl triethoxysilane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then adding 2 parts of N- (2-aminoethyl) -aminopropyltriethoxysilane, and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
EXAMPLE 121 parts of Cross-linking agent vinyltrimethoxysilane +2 parts of silane coupling agent N- (2-aminoethyl) -aminopropylmethyldimethoxysilane
The preparation method of the water-based silicone adhesive comprises the steps of firstly adding 1 part of vinyl trimethoxy silane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then adding 2 parts of 3-glycidoxypropyltrimethoxysilane, and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
EXAMPLE 131 parts of crosslinker styrene Ethyl methyl Dimethoxysilane +2 parts of silane coupling agent N- (2-aminoethyl) -aminopropyl methyl Dimethoxysilane
The preparation method of the water-based silicone adhesive of the embodiment is that 1 part of styrene ethyl methyl dimethoxy silane is added into 100 parts of 50% hydroxyl silicone oil emulsion and stirred; then adding 2 parts of 3-glycidoxypropyltrimethoxysilane, and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
EXAMPLE 141 parts of crosslinker vinyltriethoxysilane +2 parts of silane coupling agent N- (2-aminoethyl) -aminopropylmethyldimethoxysilane
The preparation method of the water-based silicone adhesive comprises the following steps of firstly adding 1 part of vinyltriethoxysilane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then adding 2 parts of 3-glycidoxypropyltrimethoxysilane, and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
EXAMPLE 151 parts of crosslinker vinylmethyldiethoxysilane +2 parts of silane coupling agent N- (2-aminoethyl) -aminopropylmethyldimethoxysilane
The preparation method of the water-based silicone adhesive of the embodiment is that 1 part of vinyl methyl diethoxysilane is added into 100 parts of 50% hydroxyl silicone oil emulsion and stirred; then adding 2 parts of 3-glycidoxypropyltrimethoxysilane, and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
EXAMPLE 161 parts of crosslinker methyltriethoxysilane +2 parts of silane coupling agent N- (2-aminoethyl) -aminopropylmethyldimethoxysilane
The preparation method of the water-based silicone adhesive comprises the following steps of firstly adding 1 part of methyl triethoxysilane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then adding 2 parts of 3-glycidoxypropyltrimethoxysilane, and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
EXAMPLE 171 parts of crosslinker methyltrimethoxysilane +2 parts of silane coupling agent N- (2-aminoethyl) -aminopropylmethyldimethoxysilane
The preparation method of the water-based silicone adhesive comprises the steps of firstly adding 1 part of methyltrimethoxysilane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then adding 2 parts of 3-glycidoxypropyltrimethoxysilane, and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
EXAMPLE 181 parts of crosslinker methylethyldimethoxysilane +2 parts of silane coupling agent N- (2-aminoethyl) -aminopropylmethyldimethoxysilane
The preparation method of the water-based silicone adhesive of the embodiment is that 1 part of methyl ethyl dimethoxy silane is added into 100 parts of 50% hydroxyl silicone oil emulsion and stirred; then adding 2 parts of 3-glycidoxypropyltrimethoxysilane, and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
Example 19 the catalyst was dibutyl tin dilaurate
The preparation method of the water-based silicone adhesive comprises the steps of firstly adding 1 part of styrene ethyl triethoxysilane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then adding 2 parts of 3-glycidoxypropyltrimethoxysilane, and stirring; then 0.5 part of dibutyl tin dilaurate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
Example 20 catalyst tetrabutyl titanate
The preparation method of the water-based silicone adhesive comprises the steps of firstly adding 1 part of styrene ethyl triethoxysilane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then adding 2 parts of 3-glycidoxypropyltrimethoxysilane, and stirring; then adding 0.5 part of tetrabutyl titanate and stirring; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
Example 20 the catalyst is a titanium complex
The preparation method of the water-based silicone adhesive comprises the steps of firstly adding 1 part of styrene ethyl triethoxysilane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then adding 2 parts of 3-glycidoxypropyltrimethoxysilane, and stirring; then adding 0.5 part of titanium complex and stirring; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silicon micropowder, stirring and defoaming to prepare the water-based silicone adhesive.
Example 21 stability, shelf life, adhesion test to RTV Silicone adhesive
The stability, shelf life, and adhesion tests of RTV silicone adhesive were performed on the water-based silicone adhesives prepared in examples 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, and 20, respectively. The adhesion of the RTV silicone adhesive is tested according to GB/T13477.18-2002 and GB/T528-2009, and the peel adhesion and tensile strength are tested, with the test results shown in Table 1.
TABLE 1 stability, shelf life, adhesion test to RTV Silicone adhesive
As can be seen from Table 1, after the filler is added into 1 part of the cross-linking agent and 0 part of the silane coupling agent in example 1, the water is not volatilized, the system is directly agglomerated, the stability and the caking property are poor, and the quality guarantee period is short; as in example 2, 4 parts of cross-linking agent, 0 part of silane coupling agent and filler are added, the system does not stick to aluminum sheets and the like, and the aluminum sheets and the like are cured and cracked within one month, so that the quality guarantee period is short, and the stability and the caking property are poor; as in example 3, the adhesive prepared from 1 part of cross-linking agent and 2 parts of silane coupling agent does not crack, can be adhered to silicon adhesive for glass sheet aluminum sheets and the like, has a shelf life of more than one year, good stability and adhesiveness, best adhesiveness to RTV silicon adhesive, and highest peel strength and tensile strength which reach 2.67N/mm and 0.62MPa respectively, the mass ratio of the cross-linking agent to the silane coupling agent has a very large influence on the preparation of the water-based silicon adhesive, and the ratio of the cross-linking agent to the silane coupling agent is most suitable for 1 part of cross-linking agent to 2 parts of silane coupling agent. As can be seen from example 4, when an oily silane coupling agent is used, the water is not completely evaporated and the system begins to cake, resulting in poor system stability, short shelf life, poor adhesion and very poor adhesion to RTV silicone adhesives. From the comparison between examples 5, 6, 7, 8, 9, 10 and 11 and example 3, it can be seen that when 8 kinds of waterborne silane coupling agents selected by the invention are used, the performance of the prepared waterborne silicone adhesive is excellent, but the adhesion to RTV silicone adhesive is still different, and the best silane coupling agent is 3-glycidoxypropyltrimethoxysilane. From the comparison of examples 12, 13, 14, 15, 16 and 17 with example 3, it can be seen that the aqueous silicone adhesive prepared by using 8 selected cross-linking agents of the present invention is also stable in performance, but has a difference in adhesion to RTV silicone adhesive, and the best cross-linking agent is styrene ethyl triethoxysilane. Meanwhile, the influence of the silane coupling agent on the adhesion can be obviously seen, and the selection of the silane coupling agent is more important to the invention. From a comparison of examples 18, 19 and 20 with example 3, it can be seen that the 4 catalysts selected according to the invention give waterborne silicone adhesives with excellent properties, with no significant difference, but with a difference in adhesion to RTV silicone adhesives, the most preferred catalyst being diisopropyl di (acetoacetate) titanate.
EXAMPLE 22 selection of the amount of crosslinker added
The preparation method of the water-based silicone adhesive comprises the steps of firstly adding a cross-linking agent of styrene ethyl triethoxysilane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then adding 2 parts of 3-glycidoxypropyltrimethoxysilane, and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding 5 parts of precipitated white carbon black and 2 parts of fumed silica, stirring and defoaming; and finally, adding 10 parts of ground calcium carbonate and 20 parts of silica micropowder, stirring and defoaming. The crosslinking agent is added according to the table 2, the performances of the obtained water-based silicone adhesive are shown in the table 2, and the strength performance is tested according to GB/T528-1992.
TABLE 2 influence of different crosslinking Agents and amounts added
As can be seen from Table 2, 0.1 to 5 parts of the cross-linking agent can basically meet the requirements for preparing the water-based silicone adhesive, but the strength of the prepared water-based silicone adhesive is slightly weaker when the addition amount of the cross-linking agent is 0.1 to 0.5 parts, but the strength of the prepared water-based silicone adhesive is stronger and can be sufficiently met when the addition amount of the cross-linking agent is more than 1 part, so that the addition amount of the cross-linking agent of 1 part is enough.
Example 23 influence of type and quality ratio of white carbon Black on thixotropy
The preparation method of the water-based silicone adhesive comprises the steps of firstly adding 1 part of styrene ethyl triethoxysilane into 100 parts of 50% hydroxyl silicone oil emulsion, and stirring; then adding 2 parts of 3-glycidoxypropyltrimethoxysilane, and stirring; then 0.5 part of diisopropyl di (ethyl acetoacetate) titanate is added and stirred; then adding white carbon black according to the table 3, stirring and defoaming; finally, 10 parts of ground calcium carbonate and 20 parts of silica powder are added, stirred and defoamed to obtain the water-based silicone adhesive with different performances, which is specifically shown in table 3.
TABLE 3 influence of the type and mass ratio of white carbon black on thixotropy
| Sample set | Precipitated white carbon black | Fumed silica | Performance of water silicone adhesive |
| 1 | 8 | 0 | The glue is very thick but does not touch |
| 2 | 0 | 6 | The glue has good thixotropy but is easy to crack after dehydration and solidification |
| 3 | 8 | 1 | The glue is very thick and the thixotropy is poor |
| 4 | 5 | 2 | The glue has good thixotropy and does not crack after being cured |
| 5 | 1 | 6 | The glue has good thixotropy, but occasionally cracks after dehydration and solidification |
According to the table 3, the thixotropy of the water-based silicone adhesive and the gas-phase white carbon black are closely related, but the thixotropy of the gas-phase white carbon black which is singly used is excellent, and the water-based silicone adhesive is easy to crack after being cured; the precipitated white carbon black is added independently, and the water-based silicone adhesive is very thick but has no thixotropy; when 8 parts of precipitated white carbon black and 1 part of fumed silica are added simultaneously, the thixotropic property is still poor, and the requirement of coating RTV silicone adhesive cannot be met; when 1 part of precipitated white carbon black and 6 parts of fumed silica are added simultaneously, the thixotropy of the water-based silicone adhesive becomes good, but the water-based silicone adhesive still cracks occasionally after being cured, and the performance is poor; when 5 parts of precipitated white carbon black and 2 parts of fumed silica are added simultaneously, the prepared waterborne silicone adhesive has good thixotropy, does not crack after being cured, can meet the requirement of coating RTV silicone adhesive, can be coated on a vertical surface or the lower surface of the top, and does not generate sagging phenomenon. Experiments prove that the mass ratio of the precipitated white carbon black to the gas-phase white carbon black is 5 parts: the best effect is achieved when 2 parts of the active ingredients are used.
Although the present invention is disclosed above, the present invention is not limited thereto. Various changes and modifications may be effected therein by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (4)
1. The water-based silicone adhesive which can be used for bonding RTV silicone adhesive, has good thixotropy and can be used as a turnover adhesive of mildewed or yellowed RTV silicone adhesive is characterized by comprising 100 parts of 50 percent hydroxyl silicone oil emulsion, 1 part of cross-linking agent, 2 parts of silane coupling agent, 0.01-1 part of catalyst and filler by mass;
wherein the silane coupling agent is 3-glycidoxypropyltrimethoxysilane; the cross-linking agent is styrene ethyl triethoxysilane; the catalyst is diisopropyl di (ethyl acetoacetate) titanate; the filler is 1-10 parts of precipitated white carbon black, 1-10 parts of gas-phase white carbon black, 1-50 parts of ground calcium carbonate and 1-100 parts of silicon micropowder; the mass ratio of the precipitated white carbon black to the fumed white carbon black is 5 parts: and 2 parts.
2. The water-based silicone adhesive according to claim 1, wherein the water-based silicone adhesive comprises 100 parts of 50% hydroxyl silicone oil emulsion, 1 part of cross-linking agent, 2 parts of silane coupling agent, 0.5 part of catalyst, 5 parts of precipitated silica, 2 parts of fumed silica, 10 parts of ground calcium carbonate and 20 parts of silica micropowder.
3. The aqueous silicone adhesive according to claim 2, wherein the aqueous silicone adhesive further comprises a toner and/or a mold inhibitor.
4. The mixture is composed of 100 parts of 50% hydroxyl silicone oil emulsion, 1 part of cross-linking agent, 2 parts of silane coupling agent, 0.01-1 part of catalyst and filler; wherein the silane coupling agent is 3-glycidoxypropyltrimethoxysilane; the cross-linking agent is styrene ethyl triethoxysilane; the catalyst is diisopropyl di (ethyl acetoacetate) titanate; the filler is 1-10 parts of precipitated white carbon black, 1-10 parts of gas-phase white carbon black, 1-50 parts of ground calcium carbonate and 1-100 parts of silicon micropowder; the mass ratio of the precipitated white carbon black to the fumed white carbon black is 5 parts: 2 parts of (1); the preparation method of the mixture comprises the following steps of firstly, adding a cross-linking agent into the hydroxyl silicone oil emulsion, and stirring; then adding a coupling agent and stirring; adding a catalyst and stirring; adding precipitated white carbon black and gas-phase white carbon black, stirring and defoaming; and finally adding heavy calcium carbonate and silica micropowder, stirring and defoaming.
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